TY - JOUR
T1 - Synthesis, Crystal Structure, and Potentiometry of Pyridine-Containing Tetraaza Macrocyclic Ligands with Acetate Pendant Arms
AU - Kim, Won D.
AU - Hrncir, Duane C.
AU - Kiefer, Garry E.
AU - Sherry, A. Dean
PY - 1995/4/1
Y1 - 1995/4/1
N2 - Tetraazamacrocycles containing the pyridine moiety as part of the cyclic backbone and acetate pendant arms were prepared. The resulting products were characterized by high resolution NMR (1H and 13C) spectroscopy and single-crystal X-ray diffraction. Single-crystal X-ray diffraction data were obtained for the following compounds: py[12]aneN4-HCl, C1H19N4CI, orthorhombic Pnma (No. 62), a = 10.304(6) Å, b = 9.160(2) Å, c = 13.552(2) Å, Z = 4, Mo Ka, λ = 0.710 69, R = 0.037, Rw = 0.036; and BP2A·2HC1·3H2O, C18H22N4O4-C12·3H2O, triclinic P1 (No. 2), a = 10.201(0) Å, b = 13.267(3) Å, c = 8.612(6) Å, α = 97.676(2)°, β = 105.821(0)°, λ = 86.363(7)°, Z = 2, Mo Ka, λ = 0.710 69, R = 0.039, Rw = 0.038. In addition, protonation constants (log Kanu and metal ion stability constants (log KML) for BP2A (log Kh1−4L. = 9.57, 5.99, 2.59, 2.22; log KMgL = 8–9; log KcaL= 10.0; log KGdL = 14.5) and PC2A (log KH1−5L = 12.5, 5.75, 3,28, 2.38, ~1; log KMgL = 8.4, log KCaL = 10.0, log KGdL = 16.6) were determined using Potentiometric and NMR pH titrations. These values agree well with previously reported literature values for analogous ligand systems.
AB - Tetraazamacrocycles containing the pyridine moiety as part of the cyclic backbone and acetate pendant arms were prepared. The resulting products were characterized by high resolution NMR (1H and 13C) spectroscopy and single-crystal X-ray diffraction. Single-crystal X-ray diffraction data were obtained for the following compounds: py[12]aneN4-HCl, C1H19N4CI, orthorhombic Pnma (No. 62), a = 10.304(6) Å, b = 9.160(2) Å, c = 13.552(2) Å, Z = 4, Mo Ka, λ = 0.710 69, R = 0.037, Rw = 0.036; and BP2A·2HC1·3H2O, C18H22N4O4-C12·3H2O, triclinic P1 (No. 2), a = 10.201(0) Å, b = 13.267(3) Å, c = 8.612(6) Å, α = 97.676(2)°, β = 105.821(0)°, λ = 86.363(7)°, Z = 2, Mo Ka, λ = 0.710 69, R = 0.039, Rw = 0.038. In addition, protonation constants (log Kanu and metal ion stability constants (log KML) for BP2A (log Kh1−4L. = 9.57, 5.99, 2.59, 2.22; log KMgL = 8–9; log KcaL= 10.0; log KGdL = 14.5) and PC2A (log KH1−5L = 12.5, 5.75, 3,28, 2.38, ~1; log KMgL = 8.4, log KCaL = 10.0, log KGdL = 16.6) were determined using Potentiometric and NMR pH titrations. These values agree well with previously reported literature values for analogous ligand systems.
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U2 - 10.1021/ic00112a040
DO - 10.1021/ic00112a040
M3 - Article
AN - SCOPUS:0000808322
SN - 0020-1669
VL - 34
SP - 2225
EP - 2232
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 8
ER -